#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:50:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179939 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/34/7023402.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7023402
loop_
_publ_author_name
'Welby, Christine E.'
'Gilmartin, Luke'
'Marriott, Ryan R.'
'Zahid, Adam'
'Rice, Craig R.'
'Gibson, Elizabeth A.'
'Elliott, Paul I. P.'
_publ_section_title
;
 Luminescent biscyclometalated arylpyridine iridium(III) complexes with
 4,4'-bi-1,2,3-triazolyl ancillary ligands.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13527
_journal_page_last               13536
_journal_paper_doi               10.1039/c3dt51284c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C40 H28 F10 Ir N8 P'
_chemical_formula_weight         1033.87
_chemical_name_common            MeCN_Et2O
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.7140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7186(6)
_cell_length_b                   26.4926(9)
_cell_length_c                   9.3340(3)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      35.3363
_cell_measurement_theta_min      2.5883
_cell_volume                     3891.9(2)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'Bruker Instrument Service v2011.6.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36360
_diffrn_reflns_theta_full        35.63
_diffrn_reflns_theta_max         35.63
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    3.562
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.124
_refine_diff_density_min         -0.987
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         8969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0251P)²+1.9130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0524
_reflns_number_gt                8008
_reflns_number_total             8969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51284c.txt
_cod_data_source_block           I
_cod_database_code               7023402
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Ir Ir1 0.5 0.278352(3) 0.75 0.01734(2) Uani d S 1
P P1 0.5 0.43439(2) 0.25 0.03086(13) Uani d S 1
F F1 0.37236(10) 0.13962(5) 1.03934(15) 0.0517(3) Uani d . 1
F F2 0.24287(8) 0.15450(5) 0.51316(15) 0.0419(3) Uani d . 1
F F3 0.45016(10) 0.39149(5) 0.13507(15) 0.0556(4) Uani d . 1
F F4 0.42969(13) 0.43444(8) 0.3283(2) 0.0827(6) Uani d . 1
F F5 0.44924(12) 0.47683(5) 0.13446(17) 0.0643(5) Uani d . 1
N N4 0.42121(8) 0.27221(5) 0.52915(16) 0.0210(2) Uani d . 1
N N5 0.56997(8) 0.34252(5) 0.71378(15) 0.0192(2) Uani d . 1
N N6 0.63947(8) 0.34794(5) 0.67821(15) 0.0208(2) Uani d . 1
N N7 0.65158(8) 0.39771(5) 0.67468(15) 0.0216(2) Uani d . 1
C C1 0.42286(10) 0.22359(5) 0.77478(19) 0.0210(2) Uani d . 1
C C2 0.42569(11) 0.20011(7) 0.9109(2) 0.0279(3) Uani d . 1
H H2 0.4664 0.2101 1.0051 0.033 Uiso calc R 1
C C3 0.36823(13) 0.16217(7) 0.9055(2) 0.0340(4) Uani d . 1
C C4 0.30740(13) 0.14560(7) 0.7746(2) 0.0358(4) Uani d . 1
H H4 0.2691 0.1192 0.7754 0.043 Uiso calc R 1
C C5 0.30480(11) 0.16940(7) 0.6416(2) 0.0299(3) Uani d . 1
C C6 0.36080(10) 0.20790(6) 0.63704(19) 0.0235(3) Uani d . 1
C C7 0.36136(10) 0.23479(6) 0.49983(19) 0.0230(3) Uani d . 1
C C8 0.31014(12) 0.22463(7) 0.3505(2) 0.0312(3) Uani d . 1
H H8 0.2678 0.1992 0.3303 0.037 Uiso calc R 1
C C9 0.32113(14) 0.25166(8) 0.2322(2) 0.0379(4) Uani d . 1
H H9 0.2875 0.2442 0.1301 0.045 Uiso calc R 1
C C10 0.38143(14) 0.28971(8) 0.2628(2) 0.0352(4) Uani d . 1
H H10 0.3896 0.3088 0.1826 0.042 Uiso calc R 1
C C11 0.42938(11) 0.29918(7) 0.41250(19) 0.0269(3) Uani d . 1
H H11 0.4698 0.3258 0.4342 0.032 Uiso calc R 1
C C12 0.53858(9) 0.38879(5) 0.73173(17) 0.0196(2) Uani d . 1
C C13 0.59131(10) 0.42459(6) 0.70627(19) 0.0237(3) Uani d . 1
H H13 0.5865 0.4603 0.7101 0.028 Uiso calc R 1
C C14 0.72439(11) 0.41747(7) 0.6368(2) 0.0283(3) Uani d . 1
H H14A 0.7043 0.4438 0.5576 0.034 Uiso calc R 1
H H14B 0.7497 0.3899 0.5949 0.034 Uiso calc R 1
C C15 0.79118(10) 0.43949(7) 0.7745(2) 0.0270(3) Uani d . 1
C C16 0.85879(13) 0.41022(9) 0.8616(3) 0.0437(5) Uani d . 1
H H16 0.8648 0.3765 0.8324 0.052 Uiso calc R 1
C C17 0.91776(17) 0.43047(13) 0.9920(4) 0.0657(8) Uani d . 1
H H17 0.9636 0.4103 1.0531 0.079 Uiso calc R 1
C C18 0.90991(19) 0.47981(13) 1.0331(3) 0.0644(8) Uani d . 1
H H18 0.9502 0.4935 1.1226 0.077 Uiso calc R 1
C C19 0.84432(17) 0.50901(11) 0.9454(3) 0.0564(7) Uani d . 1
H H19 0.8394 0.543 0.9735 0.068 Uiso calc R 1
C C20 0.78499(13) 0.48910(8) 0.8155(3) 0.0409(5) Uani d . 1
H H20 0.7398 0.5097 0.7543 0.049 Uiso calc R 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C1 Ir1 C1 2_656 . 87.33(8)
C1 Ir1 N4 2_656 2_656 80.68(6)
C1 Ir1 N4 . 2_656 92.68(6)
C1 Ir1 N4 2_656 . 92.68(6)
C1 Ir1 N4 . . 80.68(6)
N4 Ir1 N4 2_656 . 170.87(7)
C1 Ir1 N5 2_656 . 98.54(5)
C1 Ir1 N5 . . 173.40(5)
N4 Ir1 N5 2_656 . 91.25(5)
N4 Ir1 N5 . . 95.96(5)
C1 Ir1 N5 2_656 2_656 173.40(5)
C1 Ir1 N5 . 2_656 98.54(5)
N4 Ir1 N5 2_656 2_656 95.96(5)
N4 Ir1 N5 . 2_656 91.25(5)
N5 Ir1 N5 . 2_656 75.77(6)
F4 P1 F4 2_655 . 179.89(16)
F4 P1 F5 2_655 2_655 90.17(11)
F4 P1 F5 . 2_655 89.75(10)
F4 P1 F5 2_655 . 89.75(10)
F4 P1 F5 . . 90.17(11)
F5 P1 F5 2_655 . 90.03(11)
F4 P1 F3 2_655 . 89.47(10)
F4 P1 F3 . . 90.60(10)
F5 P1 F3 2_655 . 179.32(10)
F5 P1 F3 . . 90.55(7)
F4 P1 F3 2_655 2_655 90.60(10)
F4 P1 F3 . 2_655 89.47(10)
F5 P1 F3 2_655 2_655 90.55(7)
F5 P1 F3 . 2_655 179.32(9)
F3 P1 F3 . 2_655 88.88(10)
C11 N4 C7 . . 119.28(14)
C11 N4 Ir1 . . 124.49(11)
C7 N4 Ir1 . . 115.98(11)
N6 N5 C12 . . 109.92(12)
N6 N5 Ir1 . . 134.13(10)
C12 N5 Ir1 . . 115.95(9)
N5 N6 N7 . . 105.50(11)
N6 N7 C13 . . 112.71(12)
N6 N7 C14 . . 120.07(13)
C13 N7 C14 . . 127.22(14)
C2 C1 C6 . . 118.92(14)
C2 C1 Ir1 . . 126.82(12)
C6 C1 Ir1 . . 114.25(11)
C3 C2 C1 . . 118.68(17)
C3 C2 H2 . . 120.7
C1 C2 H2 . . 120.7
F1 C3 C4 . . 117.95(16)
F1 C3 C2 . . 117.74(18)
C4 C3 C2 . . 124.31(17)
C3 C4 C5 . . 116.36(16)
C3 C4 H4 . . 121.8
C5 C4 H4 . . 121.8
F2 C5 C4 . . 116.53(15)
F2 C5 C6 . . 120.48(16)
C4 C5 C6 . . 122.96(17)
C5 C6 C1 . . 118.75(15)
C5 C6 C7 . . 125.70(16)
C1 C6 C7 . . 115.55(13)
N4 C7 C8 . . 120.06(15)
N4 C7 C6 . . 113.35(14)
C8 C7 C6 . . 126.56(15)
C9 C8 C7 . . 119.82(17)
C9 C8 H8 . . 120.1
C7 C8 H8 . . 120.1
C8 C9 C10 . . 119.80(17)
C8 C9 H9 . . 120.1
C10 C9 H9 . . 120.1
C11 C10 C9 . . 118.35(17)
C11 C10 H10 . . 120.8
C9 C10 H10 . . 120.8
N4 C11 C10 . . 122.65(17)
N4 C11 H11 . . 118.7
C10 C11 H11 . . 118.7
N5 C12 C13 . . 107.68(12)
N5 C12 C12 . 2_656 116.15(8)
C13 C12 C12 . 2_656 136.16(9)
N7 C13 C12 . . 104.19(13)
N7 C13 H13 . . 127.9
C12 C13 H13 . . 127.9
N7 C14 C15 . . 111.59(13)
N7 C14 H14A . . 109.3
C15 C14 H14A . . 109.3
N7 C14 H14B . . 109.3
C15 C14 H14B . . 109.3
H14A C14 H14B . . 108.0
C20 C15 C16 . . 119.45(19)
C20 C15 C14 . . 120.07(18)
C16 C15 C14 . . 120.48(17)
C15 C16 C17 . . 119.7(2)
C15 C16 H16 . . 120.2
C17 C16 H16 . . 120.2
C18 C17 C16 . . 120.2(3)
C18 C17 H17 . . 119.9
C16 C17 H17 . . 119.9
C19 C18 C17 . . 120.1(2)
C19 C18 H18 . . 119.9
C17 C18 H18 . . 119.9
C18 C19 C20 . . 120.1(2)
C18 C19 H19 . . 119.9
C20 C19 H19 . . 119.9
C15 C20 C19 . . 120.4(2)
C15 C20 H20 . . 119.8
C19 C20 H20 . . 119.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ir1 C1 2_656 2.0057(14)
Ir1 C1 . 2.0057(14)
Ir1 N4 2_656 2.0443(14)
Ir1 N4 . 2.0443(14)
Ir1 N5 . 2.1540(12)
Ir1 N5 2_656 2.1540(12)
P1 F4 2_655 1.5799(16)
P1 F4 . 1.5799(16)
P1 F5 2_655 1.5907(14)
P1 F5 . 1.5907(14)
P1 F3 . 1.5917(13)
P1 F3 2_655 1.5917(13)
F1 C3 . 1.365(2)
F2 C5 . 1.352(2)
N4 C11 . 1.347(2)
N4 C7 . 1.369(2)
N5 N6 . 1.3195(16)
N5 C12 . 1.3659(18)
N6 N7 . 1.3360(18)
N7 C13 . 1.3452(19)
N7 C14 . 1.4733(19)
C1 C2 . 1.401(2)
C1 C6 . 1.415(2)
C2 C3 . 1.379(2)
C2 H2 . 0.95
C3 C4 . 1.372(3)
C4 C5 . 1.379(3)
C4 H4 . 0.95
C5 C6 . 1.395(2)
C6 C7 . 1.468(2)
C7 C8 . 1.394(2)
C8 C9 . 1.380(3)
C8 H8 . 0.95
C9 C10 . 1.386(3)
C9 H9 . 0.95
C10 C11 . 1.379(3)
C10 H10 . 0.95
C11 H11 . 0.95
C12 C13 . 1.369(2)
C12 C12 2_656 1.441(3)
C13 H13 . 0.95
C14 C15 . 1.506(3)
C14 H14A . 0.99
C14 H14B . 0.99
C15 C20 . 1.383(3)
C15 C16 . 1.386(3)
C16 C17 . 1.390(4)
C16 H16 . 0.95
C17 C18 . 1.381(4)
C17 H17 . 0.95
C18 C19 . 1.366(4)
C18 H18 . 0.95
C19 C20 . 1.386(3)
C19 H19 . 0.95
C20 H20 . 0.95
